CN110865038A - Method for measuring magnesium content in zinc and zinc alloy - Google Patents
Method for measuring magnesium content in zinc and zinc alloy Download PDFInfo
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Abstract
A method for determining the magnesium content in zinc and zinc alloys comprises the following steps: weighing a sample, adding dilute hydrochloric acid into the sample, placing the sample on a low-temperature electric furnace for heating and continuously dissolving after the violent reaction of the sample is stopped until the sample is completely dissolved, and adding water after cooling at room temperature; adding an interference elimination agent into the treated sample, adopting water to perform constant volume on the mixed solution, and shaking up to obtain a sample to be detected; the flame atomic absorption spectrometer sequentially sucks the blank solution and the magnesium standard series solution, analyzes and determines a light absorption value and draws a working curve; and (4) sucking a sample to be detected, and searching the working curve of the magnesium content according to the light absorption value of the sample to be detected to obtain the magnesium content in the sample to be detected. By using LaCl3、SrCl2Or one of 8-hydroxyquinoline is used as an interference eliminator, so that the interference of aluminum on magnesium element in the light absorption value measurement can be greatly reduced; simple operation, low detection limit, high accuracy and wide linear range, and can meet the requirement of measuring magnesium in zinc and zinc alloy.
Description
Technical Field
The invention belongs to the technical field of detection methods, and relates to a method for measuring the content of magnesium in zinc and zinc alloy.
Background
The use of zinc and zinc alloy in nonferrous metals is second to copper and aluminum, and the zinc and zinc alloy is widely applied to the fields of automobiles, household appliances, light industry, machinery, batteries and the like. Generally, the mass fraction of zinc in pure zinc is 99.0-99.9%, and the highest zinc can reach 99.99%, while zinc alloy is a non-ferrous alloy formed by adding aluminum, copper, magnesium and other elements into zinc as a matrix, and can be divided into zinc-aluminum alloy and zinc-copper alloy according to the components, wherein the mass fraction of aluminum is generally 0.2-16%, the mass fraction of copper is 0.2-5.5%, iron is not more than 0.3%, and other elements are trace impurities. Although magnesium in the zinc alloy is doped as a trace element, the doping of the trace magnesium can refine the structure, thereby enhancing the strength of the alloy, and simultaneously reducing intergranular corrosion and improving the wear resistance of the alloy. However, if the content of magnesium in the zinc alloy is more than 0.08%, the toughness of the alloy is lowered, the fluidity of the alloy is deteriorated, and the alloy is liable to have unfavorable behaviors such as oxidation loss in a molten state. Magnesium is used as a necessary element in zinc alloy, so that an analysis method which is easy to operate and accurate in measurement is necessary.
Although the determination of the magnesium content in the zinc alloy has been reported, the interference of coexisting elements on magnesium elements exists in the testing process, so that the testing result is inaccurate; in addition, the measurement range of the magnesium content in the existing zinc alloy is narrow, and the application is limited.
Disclosure of Invention
The invention aims to provide a method for measuring the content of magnesium in zinc and zinc alloy, which solves the problem of inaccurate test result caused by the interference of coexisting elements in a method for measuring magnesium alloy on magnesium element.
The technical scheme adopted by the invention is as follows: a method for measuring the content of magnesium in zinc and zinc alloy comprises the following steps:
step 2, adding an interference elimination agent into the sample treated in the step 1, adopting water to perform constant volume on the mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution and a magnesium standard series solution;
step 4, the flame atomic absorption spectrometer sequentially sucks the blank solution and the magnesium standard series solution, analyzes and determines a light absorption value and draws a working curve;
and 5, sucking a sample to be detected, and searching the working curve obtained in the step 4 according to the light absorption value of the sample to be detected to obtain the magnesium content in the sample to be detected.
The invention is also characterized in that:
in the step 1, the sample weighing amount is 0.050-0.200 g, and the ratio of the sample to the dilute hydrochloric acid is 1 g: 100 mL.
In step 1, if the sample is not completely dissolved, 30% hydrogen peroxide may be added to the sample.
In the step 2, the added interference elimination agent is LaCl3、SrCl2Or 8-hydroxyquinoline.
In the step 2, the addition amount of the interference elimination agent is 5.0-20.0 mL, and the proportion of the sample to the interference elimination agent is 1 g: 100 mL.
In step 3, the specific process for preparing the blank solution is as follows:
adding 2.5-10.0 mL of dilute hydrochloric acid into a 100mL volumetric flask, wherein the ratio of the sample to the hydrochloric acid is 1 g: 50mL, adding an interference elimination agent, performing constant volume with water, and shaking up to obtain a blank solution.
The specific process for preparing the magnesium standard series solution in the step 3 comprises the following steps: adding standard solutions with different magnesium contents into a plurality of 100ml volumetric flasks, wherein the standard solutions comprise zinc alloy standard sample solutions and mixed solutions of the zinc alloy standard sample solutions and the magnesium standard solutions, then adding interference elimination agents with the same volume into each volumetric flask, and performing constant volume on the mixed solutions by adopting ultrapure water to obtain magnesium standard series solutions.
In steps 4 and 5, before the flame atomic absorption spectrometer is used for analysis, the element lamp is preheated for 5min, so that the stabilized current is 6mA, and the energy is 51 counts.
In steps 4 and 5, the working parameters of the instrument are as follows: the analysis line is 285.21nm, the slit width is 0.7nm, the absorption signal type AA, the calculation mode is Time Average, the acetylene flow is 2.50L/min, the air flow is 10.00L/min, and the measurement times are 3 times.
The invention has the beneficial effects that: the method for measuring the magnesium content in zinc and zinc alloy adopts LaCl3、SrCl2Or one of 8-hydroxyquinoline as interference eliminatorThe remover can greatly reduce the interference of aluminum on magnesium element during the measurement of light absorption value; simple operation, low detection limit, high accuracy and wide linear range, and can meet the requirement of measuring magnesium in zinc and zinc alloy.
Drawings
FIG. 1 is a graph of the working curve (SrCl) of an example of a zinc alloy in accordance with a method of the present invention for determining the magnesium content of zinc and zinc alloys2As an interference eliminator).
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a method for measuring the magnesium content in zinc and zinc alloy, which comprises the following steps:
step 2, adding 5.0-20.0 mL of interference elimination agent into the sample treated in the step 1, wherein the ratio of the sample amount to the interference elimination agent is 1 g: 100 mL. Mixing, transferring into a glass volumetric flask, performing constant volume on the mixed solution by adopting ultra-pure water, and shaking up to obtain a sample to be measured; the interference eliminator is LaCl3、SrCl2Or 8-hydroxyquinoline.
Step 3, preparing a blank solution: adding 2.5-10.0 mL of dilute hydrochloric acid into a 100mL volumetric flask, wherein the ratio of the sample to the hydrochloric acid is 1 g: 50mL, adding an interference elimination agent, performing constant volume on the mixture by using ultrapure water, and shaking up to obtain a blank sample to be detected;
step 4, preparing a magnesium standard series solution: adding standard solutions with different magnesium contents into a plurality of 100ml volumetric flasks, wherein the standard solutions comprise zinc alloy standard sample solutions and mixed solutions of the zinc alloy standard sample solutions and the magnesium standard solutions, then adding interference elimination agents with the same volume into each volumetric flask, and performing constant volume on the mixed solutions by adopting ultrapure water to obtain magnesium standard series solutions;
step 5, the flame atomic absorption spectrometer sequentially sucks a blank solution and a magnesium standard series solution, and analyzes and draws a working curve, wherein the abscissa is the concentration value of magnesium, and the ordinate is the light absorption value;
and 6, sucking the sample to be detected by the flame atomic absorption spectrometer to obtain the magnesium content of the sample to be detected, and automatically drawing a working curve according to the analysis result of the flame atomic absorption spectrometer by adopting software and displaying the magnesium content of the sample to be detected
Preheating an element lamp for 5mins before each measurement and analysis, wherein the current after stabilization is 6mA, and the energy is 51 counts; the parameters of the flame atomic absorption spectrometer are as follows: the analysis line is 285.21nm, the slit width is 0.7nm, the absorption signal type AA, the calculation mode is Time Average, the acetylene flow is 2.50L/min, the air flow is 10.00L/min, and the measurement times are 3 times.
The present invention performs the following selection test for the acid and interference eliminator for dissolving the sample:
in order to compare the effect of different sample-dissolving acids on the interference elimination agent and the influence on the determination result of the alloy sample, the invention respectively adds different types of interference elimination agents into the zinc alloy Z50 (the magnesium content is 0.0238%) sample solution dissolved by the dilute hydrochloric acid and the dilute nitric acid and performs analysis, and the determination result is shown in tables 2 and 3.
TABLE 1 test results of different interference cancellers on nitric acid dissolved zinc alloy samples
Table 2 test results of different interference cancellers on zinc alloy samples dissolved in hydrochloric acid
From the analysis results in tables 1 and 2, it can be seen that:
1) by adding different types of salt solutions into a zinc alloy sample solution, SrCl in a nitric acid medium is obtained2、LaCl3The citric acid and the ascorbic acid obviously increase the light absorption value of the magnesium element in the zinc alloy; in hydrochloric acid medium, except SrCl2、LaCl3Besides salt solutions such as citric acid and ascorbic acid, 8-hydroxyquinoline also obviously increases the light absorption value of magnesium element in the zinc alloy.
2) In this experiment, 5% hydrochloric acid (acid to water volume ratio 1: 20, the same below) is less than the absorbance (0.0063) of 5% nitric acid, and the absorbance of magnesium measured in a zinc alloy sample dissolved by hydrochloric acid is basically higher than that measured after the sample is dissolved by nitric acid under the action of the same type of salt solution, so that the action effect of hydrochloric acid is better than that of nitric acid. Therefore, hydrochloric acid dissolution was used for the experiments. In addition, physical interference of acid can be eliminated by uniformly adding acid.
Interference determination
In order to clarify the interference of the possible coexisting elements in zinc and zinc alloy to magnesium, the coexisting elements are judged to be interference. Prior to the experiment, 14 100mL volumetric flasks were prepared in advance, 1#Volumetric flask with ultrapure water as calibration blank, 2#～14#5mL of 10mg/L magnesium standard solution is added into the volumetric flask, and then the mixture is added to the flask to form a mixture with the concentration of 3#～14#The single element standard solutions with the corresponding sequence numbers in the table 4 are sequentially added into the volumetric flask, and after constant volume shaking up, analysis is performed.
The ratio of the net absorbance of the mixed solution obtained by mixing a single coexisting element with 0.5mg/L magnesium standard solution to the absorbance of the pure magnesium standard solution is recorded as an interference factor f, and the interference degree of the coexisting element on magnesium is represented by the value.
TABLE 3 interference test of pure solution of single element on magnesium
Note: the concentration of each element in the list is the concentration value of the single element in the solution at the time the measurement was performed.
As can be seen from table 3: when the magnesium element in the zinc alloy is measured, only aluminum and titanium have certain influence on the measurement of magnesium, and the influence of zinc on magnesium is mainly a matrix effect and can be eliminated by adding the zinc matrix element or establishing a working curve by adopting a zinc alloy standard sample. Therefore, the key to interference resolution is to reduce or eliminate the effect of aluminum and titanium on magnesium.
Interference cancellation
Based on the results of the previous discussion, since only aluminum and titanium interfere with magnesium in the determination of magnesium in zinc alloys, interference cancellation tests were performed on aluminum and titanium, respectively. Meanwhile, the experiment is considered to adopt hydrochloric acid to dissolve the sample, and then SrCl can be selected2、LaCl3Citric acid, ascorbic acid or 8-hydroxyquinoline as interference eliminator.
The elimination test of the aluminum element interference is carried out: 8 100mL volumetric flasks were prepared in advance, 1#Volumetric flask with ultrapure water as calibration blank, 2#～8#5mL of 10mg/L magnesium standard solution is added into the volumetric flask, and the reaction is continued to 3#～8#5mL of 1000mg/L aluminum standard solution is added into the volumetric flask, and then 4#～8#The interference elimination agents (the addition amount is 5mL) with the corresponding numbers in the table 5 are sequentially added into the volumetric flask, the analysis is carried out after constant volume shaking up, and the measurement results are shown in the table 4.
TABLE 4 suppression of the degree of aluminum interference by various interference suppressants
As can be seen from table 4: adding LaCl to an aluminum-containing analysis solution3、SrCl2And 8-hydroxyquinoline, both significantly increase the absorbance of magnesium. And comparing the results with those of the analysis of magnesium single standard solution, LaCl3And SrCl2Substantially eliminates the interference of aluminum on magnesium, and 8-Hydroxyquinoline also greatly reduces the interference of aluminum.
The elimination test of titanium interference is carried out: 8 100mL volumetric flasks were prepared in advance, 1#Volumetric flask with ultrapure water as calibration blank, 2#～8#5mL of 10mg/L magnesium standard solution is added into the volumetric flask, and the reaction is continued to 3#～8#Titanium standard solution with the concentration of 1mL and 1000mg/L is added into the volumetric flask, and then the volume is increased to 4#～8#The interference elimination agents (the addition amount is 5mL) with the corresponding numbers in the table 5 are sequentially added into the volumetric flask, the analysis is carried out after constant volume shaking up, and the measurement results are shown in the table 5.
TABLE 5 suppression of the degree of interference of different interference suppressants on titanium
As can be seen from table 5: adding LaCl into titanium-containing analysis solution3Citric acid and ascorbic acid, all increase the absorbance of magnesium and substantially eliminate the interference of titanium with magnesium.
Based on the current state of development of zinc alloys, except for the fact that the wrought zinc alloys (such as Zn-Cu-0.1Ti) contain a small amount of titanium, the content of titanium in other forms of zinc alloys is very low, and as can be seen from Table 5, the interference of titanium with magnesium at a concentration of 1.0% is small, so the influence of titanium on the measurement of magnesium can be ignored in general, and only the interference of aluminum needs to be considered. Therefore, only the LaCl is considered to be selected when determining the magnesium element in the zinc alloy3、SrCl2Or 8-hydroxyquinoline as an interference eliminator to eliminate the interference of aluminum on magnesium.
Through the way, the method for determining the magnesium content in zinc and zinc alloy adopts LaCl3、SrCl2Or one of 8-hydroxyquinoline is used as an interference eliminator, so that the interference of aluminum on magnesium element in the light absorption value measurement can be greatly reduced; simple operation, low detection limit, high accuracy and wide linear range, and can meet the requirement of measuring magnesium in zinc and zinc alloy.
Example 1
step 2, adding 10mL SrCl into the sample treated in the step 12Mixing, transferring into a glass volumetric flask, performing constant volume to 100mL by adopting ultrapure mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution: 5mL of hydrochloric acid and 10mL of SrCl were added to a 100mL volumetric flask2Carrying out constant volume on the sample by adopting ultrapure water, and shaking up the sample to obtain a blank sample to be detected;
step 4, preparing a standard sample solution: a mixture of standard solution Z48 (No. C41X GLV40, Mg: 0.0034%), Z50 (No. C43X Z60, Mg: 0.0238%), a mixture of Z48 and 5mL of 10Mg/L magnesium standard solution, a mixture of Z49 (No. C41X GLV30, Mg: 0.00145%) and 8mL10 Mg/L magnesium standard solution, and a mixture of Z50 and 10mL of 10Mg/L magnesium standard solution were sequentially added to 5 100mL volumetric flasks, and 10mL of SrCl was added to each volumetric flask2After mixing, adopting ultrapure water to perform constant volume to obtain magnesium standard series sample solutions with different gradients;
step 5, the flame atomic absorption spectrometer sequentially sucks a blank solution and a magnesium standard series solution, after analysis is finished, application software automatically draws a working curve, wherein the abscissa is the concentration value of magnesium, the ordinate is the light absorption value, and as shown in fig. 1, the linear regression equation is that A is 0.01851 + 1.08642 rho, and R is 0.9996;
step 6, then sucking 2 samples to be tested (1)#And 2#) The results are shown in Table 1, and compared with those of inductively coupled plasma atomic emission spectrometry (ICP-AES), the data are substantially the same.
TABLE 1 determination of magnesium in Zinc alloy samples (%)
Note: this test was conducted with 10mL of SrCl2As an interference eliminator.
Example 2
step 2, adding 10mL of LaCl into the sample treated in the step 13Mixing, transferring into a glass volumetric flask, performing constant volume to 100mL by adopting ultrapure mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution: 5mL of hydrochloric acid and 10mL of LaCl were added to a 100mL volumetric flask3Carrying out constant volume on the sample by adopting ultrapure water, and shaking up the sample to obtain a blank sample to be detected;
step 4, preparing a standard sample solution: a mixture of standard solution Z48 (No. C41X GLV40, Mg: 0.0034%), Z50 (No. C43X Z60, Mg: 0.0238%), a mixture of Z48 and 5mL of 10Mg/L magnesium standard solution, a mixture of Z49 (No. C41X GLV30, Mg: 0.00145%) and 8mL10 Mg/L magnesium standard solution, and a mixture of Z50 and 10mL of 10Mg/L magnesium standard solution were sequentially added to 5 100mL volumetric flasks, and 10mL of LaCl was added to each volumetric flask3After mixing, adopting ultrapure water to perform constant volume to obtain magnesium standard series sample solutions with different gradients;
step 5, the flame atomic absorption spectrometer sequentially sucks a blank solution and a magnesium standard series solution, after analysis is finished, application software automatically draws a working curve, wherein the abscissa is the concentration value of magnesium, the ordinate is the light absorption value, the linear regression equation is that A is 0.01921 + 1.47265 rho, and R is 0.9992;
step 6, then 2 samples to be tested are sucked (3)#And 4#) See Table 2, the results of which are combined with inductively coupled plasma atomic emission spectrometryThe results of measurement (ICP-AES) were compared, and the data were substantially the same.
TABLE 2 determination of magnesium in Zinc alloy samples (%)
Note: this experiment was performed with 10mL of LaCl3As an interference eliminator.
Example 3
step 2, adding 10mL of 8-hydroxyquinoline into the sample treated in the step 1, mixing, transferring into a glass volumetric flask, performing constant volume to 100mL by adopting ultra-pure mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution: adding 5mL of hydrochloric acid into a 100mL volumetric flask, adding 10mL of 8-hydroxyquinoline, performing constant volume by adopting ultrapure water, and shaking up to obtain a blank sample to be detected;
step 4, preparing a standard sample solution: adding a standard solution Z48 (numbered C41X GLV40, Mg: 0.0034%), Z50 (numbered C43X Z60, Mg: 0.0238%), a mixed solution of Z48 and 5mL of 10Mg/L magnesium standard solution, a mixed solution of Z49 (numbered C41X GLV30, Mg: 0.00145%), a mixed solution of 8mL10 Mg/L magnesium standard solution and a mixed solution of Z50 and 10mL of 10Mg/L magnesium standard solution into 5 100mL volumetric flasks in sequence, adding 10mL of 8-hydroxyquinoline into each volumetric flask, mixing, and performing constant volume on the volumetric flasks by adopting ultrapure water to obtain magnesium standard series sample solutions with different gradients;
step 5, the flame atomic absorption spectrometer sequentially sucks a blank solution and a magnesium standard series solution, after analysis is finished, application software automatically draws a working curve, wherein the abscissa is the concentration value of magnesium, the ordinate is the light absorption value, the linear regression equation is that A is 0.01766 + 1.04937 rho, and R is 0.9994;
step 6, then 2 samples to be tested are inhaled (5)#And 6#) The results are shown in Table 3, and compared with those of inductively coupled plasma atomic emission spectrometry (ICP-AES), the data are substantially the same.
TABLE 3 determination of magnesium in Zinc alloy samples (%)
Note: this experiment was conducted using 10mL of 8-hydroxyquinoline as the interference eliminator.
Example 4
step 2, adding 5mL SrCl into the sample treated in the step 12Mixing, transferring into a glass volumetric flask, performing constant volume to 100mL by adopting ultrapure mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution: 2.5mL of hydrochloric acid and 5mL of SrCl were added to a 100mL volumetric flask2Carrying out constant volume on the sample by adopting ultrapure water, and shaking up the sample to obtain a blank sample to be detected;
step 4, preparing a standard sample solution: a mixture of standard solution Z48 (No. C41X GLV40, Mg: 0.0034%), Z50 (No. C43X Z60, Mg: 0.0238%), a mixture of Z48 and 5mL of 10Mg/L magnesium standard solution, a mixture of Z49 (No. C41X GLV30, Mg: 0.00145%) and 8mL10 Mg/L magnesium standard solution, and a mixture of Z50 and 10mL of 10Mg/L magnesium standard solution were sequentially added to 5 100mL volumetric flasks, and 5mL of SrCl was added to each volumetric flask2After mixing, adopting ultrapure water to perform constant volume to obtain magnesium standards with different gradientsA series of sample solutions;
step 5, the flame atomic absorption spectrometer sequentially sucks a blank solution and a magnesium standard series solution, after analysis is finished, application software automatically draws a working curve, wherein the abscissa is the concentration value of magnesium, the ordinate is the light absorption value, the linear regression equation is that A is 0.01713 + 1.12746 rho, and R is 0.9992;
step 6, then 2 samples to be tested are aspirated (7)#And 8#) The results are shown in Table 4, and compared with those of inductively coupled plasma atomic emission spectrometry (ICP-AES), the data are substantially the same.
TABLE 4 determination of magnesium in Zinc alloy samples (%)
Note: this experiment was conducted with 5mL of SrCl2As an interference eliminator.
Example 5
step 2, adding 20mL SrCl into the sample treated in the step 12Mixing, transferring into a glass volumetric flask, performing constant volume to 100mL by adopting ultrapure mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution: to a 100mL volumetric flask was added 10mL hydrochloric acid and 20mL SrCl2Carrying out constant volume on the sample by adopting ultrapure water, and shaking up the sample to obtain a blank sample to be detected;
step 4, preparing a standard sample solution: a5 100mL volumetric flask was charged with standard solution Z48 (No. C41X GLV40, Mg: 0.0034%), Z50 (No. C43X Z60, Mg: 0.0238%), Z48 and 5mL of a 10Mg/L magnesium standard in that orderA mixture of the solutions, a mixture of Z49 (No. C41X GLV30, Mg: 0.00145%) and 8mL10 Mg/L of a magnesium standard solution, and a mixture of Z50 and 10mL10Mg/L of a magnesium standard solution, and 20mL of SrCl was added to each volumetric flask2After mixing, adopting ultrapure water to perform constant volume to obtain magnesium standard series sample solutions with different gradients;
step 5, the flame atomic absorption spectrometer sequentially sucks a blank solution and a magnesium standard series solution, after analysis is finished, application software automatically draws a working curve, wherein the abscissa is the concentration value of magnesium, the ordinate is the light absorption value, the linear regression equation is that A is 0.01754 + 1.07435 rho, and R is 0.9994;
step 6, then 2 samples to be tested are aspirated (9)#And 10#) The results are shown in Table 5, and compared with those of inductively coupled plasma atomic emission spectrometry (ICP-AES), the data are substantially the same.
TABLE 5 determination of magnesium in Zinc alloy samples (%)
Note: this experiment was conducted with 20mL of SrCl2As an interference eliminator.
Claims (9)
1. A method for measuring the content of magnesium in zinc and zinc alloy is characterized by comprising the following steps:
step 1, weighing a sample, adding dilute hydrochloric acid into the sample, after the violent reaction of the sample is stopped, placing the sample on a low-temperature electric furnace to be heated and continuously dissolved until the sample is completely dissolved, and adding water after the sample is cooled at room temperature;
step 2, adding an interference elimination agent into the sample treated in the step 1, adopting water to perform constant volume on the mixed solution, and shaking up to obtain a sample to be detected;
step 3, preparing a blank solution and a magnesium standard series solution;
step 4, the flame atomic absorption spectrometer sequentially sucks the blank solution and the magnesium standard series solution, analyzes and determines a light absorption value and draws a working curve;
and 5, sucking the sample to be detected by the flame atomic absorption spectrometer, and searching the working curve obtained in the step 4 according to the light absorption value of the sample to be detected to obtain the magnesium content in the sample to be detected.
2. The method for measuring the magnesium content in zinc and zinc alloys according to claim 1, wherein in the step 1, the sample weighing amount is 0.050 to 0.200g, and the ratio of the sample to the dilute hydrochloric acid is 1 g: 100 mL.
3. The method for determining the magnesium content in zinc and zinc alloys according to claim 1, wherein in step 1, if the sample is not completely dissolved, 30% hydrogen peroxide is added to the sample.
4. The method for determining the content of magnesium in zinc and zinc alloys according to claim 1, wherein the interference eliminator added in step 2 is LaCl3、SrCl2Or 8-hydroxyquinoline.
5. The method for determining the content of magnesium in zinc and zinc alloy according to claim 1, wherein in the step 2, the addition amount of the interference elimination agent is 5.0-20.0 mL, and the ratio of the sample to the interference elimination agent is 1 g: 100 mL.
6. The method for measuring the magnesium content in zinc and zinc alloy according to claim 1, wherein the specific process for preparing the blank solution in the step 3 is as follows:
adding 2.5-10.0 mL of dilute hydrochloric acid into a 100mL volumetric flask, wherein the ratio of the sample to the hydrochloric acid is 1 g: 50mL, adding an interference elimination agent, performing constant volume with water, and shaking up to obtain a blank solution.
7. The method for measuring the magnesium content in zinc and zinc alloy according to claim 1, wherein the specific process for preparing the magnesium standard series solution in the step 3 is as follows: adding standard solutions with different magnesium contents into a plurality of 100ml volumetric flasks, wherein the standard solutions comprise zinc alloy standard sample solutions and mixed solutions of the zinc alloy standard sample solutions and the magnesium standard solutions, then adding interference elimination agents with the same volume into each volumetric flask, and performing constant volume on the mixed solutions by adopting ultrapure water to obtain magnesium standard series solutions.
8. The method of claim 1, wherein in steps 4 and 5, the elemental lamp is preheated for 5min before the flame atomic absorption spectrometer analysis, so that the stabilized current is 6mA and the energy is 51 counts.
9. The method for measuring the content of magnesium in zinc and zinc alloy according to claim 1, wherein in the steps 4 and 5, the working parameters of the instrument are as follows: the analysis line is 285.21nm, the slit width is 0.7nm, the absorption signal type AA, the calculation mode is TimeAverage, the acetylene flow is 2.50L/min, the air flow is 10.00L/min, and the measurement times are 3 times.
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| US20110027895A1 (en) * | 2008-04-08 | 2011-02-03 | Southwest Aluminium (Group) Co., Ltd. | Determination method of magnesium content in aluminium alloy |
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